Synthesis and Characterization of a Novel Charring Agent and Its Application in Intumescent Flame Retardant Polypropylene System

A novel halogen-free charring agent bi(4-methoxy-1-phospha-2, 6, 7-trioxabicyclo [2.2.2]-octane-1-sulfide) phenylphosphate (BSPPO) was synthesized from phenylphosphonic dichloride (PPDC), and 4-hydroxymethyl-1-phospha-2, 6, 7-trioxabicyclo[2.2.2]-octane-1-sulfide (SPEPA) which was synthesized from pentaerythritol and thiophosphoryl chloride in this article. The structure of BSPPO and SPEPA was characterized by Fourier transform infrared (FTIR), H-1-NMR, C-13-NMR, and P-31-NMR. Combined with ammonium polyphosphate (APP) and melamine pyrophosphate (MPP), the flame retardance and dripping resistance of BSPPO added in polypropylene (PP) were investigated. The fire performance of the flame retardant PP system was investigated by limiting oxygen index (LOI), vertical burning test (UL-94), and cone calorimeter. The thermal stabilities of the composites were studied by thermogravimetric analysis (TGA). The flame retardance mechanism was investigated by FTIR and scanning electronic micrograph (SEM). The mechanical properties and water solubility were also investigated. The residue of BSPPO is 40.6% at 600 degrees C, which indicates BSPPO has excellent charring ability. The char residue of the polypropylene intumescent flame retardant (PP-IFR) system is 22% at 600 degrees C, which suggests that the flame retardation synergy of APP, BSPPO, and MPP is good. With the optimum formulation, the LOI of the IFR-PP system is 32.0, and the UL-94 is V-0 rating. The heat release rate (HRR), total heat release (THR), smoke production rate (SPR), total smoke production (TSP), and mass loss rate (MLR) of IFR-PP with the optimum formulation decrease significantly comparing to pure PP from cone calorimeter analysis. The FTIR and SEM results indicate that the char properties and the char yield have direct effect on the flame retardance and antidripping behaviors. (C) 2011 Wiley Periodicals, Inc. J Appl Polym Sci 123: 1636-1644, 2012